食品与发酵科技
食品與髮酵科技
식품여발효과기
SICHUAN FOOD AND FERMENTATION
2014年
3期
75-78
,共4页
倪永付%王勇%闫秋成%朱莉萍
倪永付%王勇%閆鞦成%硃莉萍
예영부%왕용%염추성%주리평
分散固相萃取%气相色谱-质谱/质谱法%蒜粉%有机磷%残留
分散固相萃取%氣相色譜-質譜/質譜法%蒜粉%有機燐%殘留
분산고상췌취%기상색보-질보/질보법%산분%유궤린%잔류
dispersive solid-phase extraction%GC-MS/MS%garlic powder%organophosphorus pesticide%residues
建立了分散固相萃取-气相色谱-串联质谱法检测蒜粉中13种有机磷农药残留的方法。样品经0.1%乙酸-乙腈提取,C18净化粉净化后,氮气吹干,用1.0mL乙酸乙酯定容,上机检测。采用TR-5MS(30m×0.25mm×25μm)色谱柱分离,在选择反应监测模式下检测,外标法定量。结果表明:13种有机磷农药在浓度0.02-1.0mg/L范围内线性关系良好,相关系数r=0.9910-0.9978,方法检测限为0.001-0.01mg/kg,定量限为0.005-0.02mg/kg。在不同添加水平下,其平均回收率为70-120%,变异系数为3.4-14.3%。
建立瞭分散固相萃取-氣相色譜-串聯質譜法檢測蒜粉中13種有機燐農藥殘留的方法。樣品經0.1%乙痠-乙腈提取,C18淨化粉淨化後,氮氣吹榦,用1.0mL乙痠乙酯定容,上機檢測。採用TR-5MS(30m×0.25mm×25μm)色譜柱分離,在選擇反應鑑測模式下檢測,外標法定量。結果錶明:13種有機燐農藥在濃度0.02-1.0mg/L範圍內線性關繫良好,相關繫數r=0.9910-0.9978,方法檢測限為0.001-0.01mg/kg,定量限為0.005-0.02mg/kg。在不同添加水平下,其平均迴收率為70-120%,變異繫數為3.4-14.3%。
건립료분산고상췌취-기상색보-천련질보법검측산분중13충유궤린농약잔류적방법。양품경0.1%을산-을정제취,C18정화분정화후,담기취간,용1.0mL을산을지정용,상궤검측。채용TR-5MS(30m×0.25mm×25μm)색보주분리,재선택반응감측모식하검측,외표법정량。결과표명:13충유궤린농약재농도0.02-1.0mg/L범위내선성관계량호,상관계수r=0.9910-0.9978,방법검측한위0.001-0.01mg/kg,정량한위0.005-0.02mg/kg。재불동첨가수평하,기평균회수솔위70-120%,변이계수위3.4-14.3%。
A method was established to determine the 13 organophosphorus pesticide residues in garlic powder by dispersive solid-phase extraction and gas chromatography-tandem mass spectrometry method. The sample was ex-tracted by 0.1% acetic acid-acetonitrile. After being cleaned by C18 powder, and then dried by the nitrogen flow, the sample was dissolved in 1.0mL ethyl acetate and performed on TR-5MS (30m×0.25mm×25μm) column. The analysis was carried out in the select reaction monitoring mode and external standard method was used for quantifi-cation. The calibration curve of the 13 organophosphorus pesticides was good linear from 0.02 to 1.0mg/L with the correlation coefficient r=0.9910-0.9978, the detection limits of this method were 0.001~0.01mg/kg and the quantita-tive limits were 0.005-0.02mg/kg. In different concentrations, the average recoveries of this method were 70-120%and the variability coefficient were 3.4-14.3%.